Name: Hydrogen Charging of Aluminum using Friction in Water (Video) | JoVE Journal
Uploaded: 2020-01-28T14:30:00.000+00:00
Duration: 7 min 50 s
Description: Learn a novel friction-in-water method to charge aluminum alloys with hydrogen, overcoming surface oxide film challenges. This technique enables efficient hydrogen storage and embrittlement studies in materials science.

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5 minutes

This work was financially supported in part by The Light Metal Educational Foundation, Inc., Osaka, Japan

1. Material preparation
<ol>
	<li>Use 1 mm thick plates made of an aluminum-magnesium-silicon alloy containing 1 mass% Mg and 0.8 mass% Si (Al-Mg-Si).</li>
	<li>Make test pieces from the Al-Mg-Si alloy plates having a gauge length of 10 mm and width of 5 mm.</li>
	<li>Anneal the test pieces at 520 &#730;C for 1 h using an air furnace. Quench in water as a solution heat treatment.</li>
	<li>Anneal the test pieces at 175 &#730;C for 18 h as a peak aging heat treatment (T6-temper).</li>
	<li>Polish the surface of the test pieces using silicon carbide emery paper (#2000) without water.</li>
	<li>Measure the weight of the polished specimens to a precision of 0.0001 g using an electric balance</li>
	<li>Measure the thickness and width of the gauge part of the specimens to a precision of 0.001 mm using an optical comparator.</li>
</ol>
2. FW procedure (Figure 1)
<ol>
	<li>Attach two Al-Mg-Si alloy specimens using glue to a triangular, prism-shaped stirrer made by a fluorocarbon polymer.</li>
	<li>Prepare a cylinder glass container with an empty top as a reaction vessel.</li>
	<li>Attach a round polishing paper made by silicon carbides, #2000 with a diameter of 10 mm, using double sided tape in the bottom inside of the container.</li>
	<li>Place the triangular, prism-shaped stirrer with two specimens on the polishing paper at the bottom surface of the glass container.</li>
	<li>Pour 100 mL of distilled water into the glass container from the top.</li>
	<li>Cover the glass container with a round rubber piece with three holes (for a gas inlet, for a gas outlet, and for a pH probe at the top of the glass container).</li>
	<li>Fill the glass container with high purity (99.999%) argon at a constant flow rate of 20 mL/min after closing the rubber cover.</li>
	<li>Connect the gas outlet to a gas chromatograph (GC) with a semiconductor hydrogen sensor (detection limit: 5 ppb).</li>
	<li>Wait until the gas in the container is replaced by argon.</li>
	<li>Rotate the triangular, prism-shaped stirrer with two specimens on a magnetic stirrer with a constant rotating speed at room temperature.</li>
	<li>Measure the hydrogen generation during the stirrer rotation using the GC, taking one measurement every 2 min.</li>
	<li>Measure the pH of the water in the container during the stirrer rotation.</li>
	<li>Remove the two specimens from the triangular, prism-shaped stirrer by immersion in acetone with an ultrasonic vibration for 5 min after the FW procedure.</li>
	<li>Measure the weight and thickness of the specimens again after the FW procedure using the electric balance and an optical comparator, respectively.</li>
</ol>
3. Hydrogen absorption by the FW procedure
<ol>
	<li>After the FW procedure, cut a specimen to a rectangular shape of 1 x 5 x 10 mm.</li>
	<li>Place the specimen inside a quartz tube with a diameter of 10 mm connected to a GC with a semiconductor hydrogen sensor.</li>
	<li>Flow high purity (99.999%) argon gas in a quartz tube with a constant flow rate of 20 mL/min.</li>
	<li>Heat the quartz tube with the specimen using a tubular furnace at a constant heating rate, 200 &#730;C/h.</li>
	<li>Measure the thermal hydrogen desorption of the specimen after the FW procedure using the GC.</li>
</ol>
4. Material evaluation after the FW procedure
<ol>
	<li>Carry out tensile tests (at least 3x, to ensure repeatability) in laboratory air with a crosshead speed of 2 mm/min using a specimen that has been treated by the FW procedure.</li>
	<li>Measure the tensile properties (e.g., tensile strength, fracture strain) obtained from the stress-strain curve in the tensile test.</li>
	<li>Observe the fracture behavior with a secondary electron microscope (SEM) after the tensile test.</li>
</ol>

<ol><li>Horikawa, K., Matsubara, T., Kobayashi, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Hydrogen+charging+of+Al-Mg-Si-based+alloys+by+friction+in+water+and+its+effect+on+tensile+properties%5BTitle%5D)+AND+%22Materials+Science+and+Engineering+A%22%5BJournal%5D)">Hydrogen charging of Al-Mg-Si-based alloys by friction in water and its effect on tensile properties.</a> Materials Science and Engineering A. 764, 138199(2019).</li>
<li>Horikawa, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Current+research+trends+in+aluminum+alloys+for+a+high-pressure+hydrogen+gas+container%5BTitle%5D)+AND+%22Journal+of+Japan+Institute+of+Light+Metals%22%5BJournal%5D)">Current research trends in aluminum alloys for a high-pressure hydrogen gas container.</a> Journal of Japan Institute of Light Metals. 60, 542-547 (2010).</li>
<li>Kuramoto, S., Hsieh, M. C., Kanno, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Environmental+embrittlement+of+Al-Mg-Si+base+alloys+deformed+at+low+strain+rates+in+laboratory+air%5BTitle%5D)+AND+%22Journal+of+Japan+Institute+of+Light+Metals%22%5BJournal%5D)">Environmental embrittlement of Al-Mg-Si base alloys deformed at low strain rates in laboratory air.</a> Journal of Japan Institute of Light Metals. 52, 250-255 (2002).</li>
<li>Horikawa, K., Yoshida, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Visualization+of+Hydrogen+in+Tensile-Deformed+Al-5%25Mg+Alloy+by+means+of+Hydrogen+Microprint+Technique+with+EBSP+Analysis%5BTitle%5D)+AND+%22Materials+Transactions%22%5BJournal%5D)">Visualization of Hydrogen in Tensile-Deformed Al-5%Mg Alloy by means of Hydrogen Microprint Technique with EBSP Analysis.</a> Materials Transactions. 45, 315-318 (2004).</li>
<li>Ueda, K., Horikawa, K., Kanno, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Suppression+of+high+temperature+embrittlement+of+Al-5%25Mg+alloys+containing+a+trace+of+sodium+caused+by+antimony+addition%5BTitle%5D)+AND+%22Scripta+Materialia%22%5BJournal%5D)">Suppression of high temperature embrittlement of Al-5%Mg alloys containing a trace of sodium caused by antimony addition.</a> Scripta Materialia. 37, 1105-1110 (1996).</li>
<li>Horikawa, K., Ando, N., Kobayashi, H., Urushihara, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Visualization+of+hydrogen+gas+evolution+during+deformation+and+fracture+in+SCM+440+steel+with+different+tempering+conditions%5BTitle%5D)+AND+%22Materials+Science+and+Engineering+A%22%5BJournal%5D)">Visualization of hydrogen gas evolution during deformation and fracture in SCM 440 steel with different tempering conditions.</a> Materials Science and Engineering A. 534, 495-503 (2012).</li>
<li>Horikawa, K., Yamada, H., Kobayashi, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Effect+of+strain+rate+on+hydrogen+gas+evolution+behavior+during+tensile+deformation+in+6061+and+7075+aluminum+alloys%5BTitle%5D)+AND+%22Journal+of+Japan+Institute+of+Light+Metals%22%5BJournal%5D)">Effect of strain rate on hydrogen gas evolution behavior during tensile deformation in 6061 and 7075 aluminum alloys.</a> Journal of Japan Institute of Light Metals. 62, 306-312 (2012).</li>
<li>Horikawa, K., Okada, H., Kobayashi, H., Urushihara, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Visualization+of+diffusive+hydrogen+in+low+alloy+steel+by+means+of+hydrogen+microprint+technique+at+elevated+temperatures%5BTitle%5D)+AND+%22Materials+Transactions%22%5BJournal%5D)">Visualization of diffusive hydrogen in low alloy steel by means of hydrogen microprint technique at elevated temperatures.</a> Materials Transactions. 50, 759-764 (2009).</li>
<li>Horikawa, K., Okada, H., Kobayashi, H., Urushihara, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Visualization+of+hydrogen+during+fatigue+fracture+in+an+Al-Mg-Si+alloy%5BTitle%5D)+AND+%22Journal+of+Japan+Institute+of+Light+Metals%22%5BJournal%5D)">Visualization of hydrogen during fatigue fracture in an Al-Mg-Si alloy.</a> Journal of Japan Institute of Light Metals. 56, 210-213 (2006).</li>
<li>Horikawa, K., Okada, H., Kobayashi, H., Urushihara, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Visualization+of+hydrogen+distribution+in+tensile-deformed+Al-5%25Mg+alloy+investigated+by+means+of+hydrogen+microprint+technique+with+EBSP%5BTitle%5D)+AND+%22Journal+of+the+Japan+Institute+of+Metals%22%5BJournal%5D)">Visualization of hydrogen distribution in tensile-deformed Al-5%Mg alloy investigated by means of hydrogen microprint technique with EBSP.</a> Journal of the Japan Institute of Metals. 68, 1043-1046 (2004).</li>
<li>Yamada, H., Tsurudome, M., Miura, N., Horikawa, K., Ogasawara, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Ductility+loss+of+7075+aluminum+alloys+affected+by+interaction+of+hydrogen%2C+fatigue+deformation%2C+and+strain+rate%5BTitle%5D)+AND+%22Materials+Science+and+Engineering+A%22%5BJournal%5D)">Ductility loss of 7075 aluminum alloys affected by interaction of hydrogen, fatigue deformation, and strain rate.</a> Materials Science and Engineering A. 642, 194-203 (2015).</li>
<li>Toda, H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Effects+of+hydrogen+micro+pores+on+mechanical+properties+in+a+2024+aluminum+alloys%5BTitle%5D)+AND+%22Materials+Transactions%22%5BJournal%5D)">Effects of hydrogen micro pores on mechanical properties in a 2024 aluminum alloys.</a> Materials Transactions. 54, 2195-2201 (2013).</li>
<li>Yamada, H., Horikawa, K., Matsumoto, T., Kobayashi, H., Ogasawara, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Hydrogen+evolution+behavior+of+tensile+deformation+process+in+6061+and+7075+aluminum+alloys%5BTitle%5D)+AND+%22Journal+of+Japan+Institute+of+Light+Metals%22%5BJournal%5D)">Hydrogen evolution behavior of tensile deformation process in 6061 and 7075 aluminum alloys.</a> Journal of Japan Institute of Light Metals. 61, 297-302 (2011).</li>
<li>Horikawa, K., Kobayashi, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Hydrogen+absorption+of+pure+aluminum+by+friction+of+the+surface+in+water+and+its+effect+on+tensile+properties%5BTitle%5D)+AND+%22Journal+of+the+Japan+Institute+of+Metals%22%5BJournal%5D)">Hydrogen absorption of pure aluminum by friction of the surface in water and its effect on tensile properties.</a> Journal of the Japan Institute of Metals. 84, (2020).</li>
<li>Suzuki, H., Kobayashi, D., Hanada, N., Takai, K., Hagihara, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Existing+state+of+hydrogen+in+electrochemically+charged+commercial-purity+aluminum+and+its+effects+on+tensile+properties%5BTitle%5D)+AND+%22Materials+Transactions%22%5BJournal%5D)">Existing state of hydrogen in electrochemically charged commercial-purity aluminum and its effects on tensile properties.</a> Materials Transactions. 52, 1741-1747 (2011).</li>
<li>Horikawa, K., Hokazono, S., Kobayashi, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Synchronized+monitoring+between+hydrogen+gas+release+and+progress+of+atmospheric+hydrogen+embrittlement+in+7075+aluminum+alloy%5BTitle%5D)+AND+%22Journal+of+Japan+Institute+of+Light+Metals%22%5BJournal%5D)">Synchronized monitoring between hydrogen gas release and progress of atmospheric hydrogen embrittlement in 7075 aluminum alloy.</a> Journal of Japan Institute of Light Metals. 66, 77-83 (2016).</li>
<li>Manaka, T., Aoki, M., Itoh, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Thermal+desorption+spectroscopy+study+on+the+hydrogen+behavior+in+a+plasma-charged+aluminum%5BTitle%5D)+AND+%22Materials+Science+Forum%22%5BJournal%5D)">Thermal desorption spectroscopy study on the hydrogen behavior in a plasma-charged aluminum.</a> Materials Science Forum. 879, 1220-1225 (2016).</li>
<li>Ellingham, H. J. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Reducibility+of+oxides+and+sulphides+in+metallurgical+processes%5BTitle%5D)+AND+%22Journal+of+the+Society+of+Chemical+Industry%22%5BJournal%5D)">Reducibility of oxides and sulphides in metallurgical processes.</a> Journal of the Society of Chemical Industry. 63, 125-133 (1944).</li>
<li>Pourbaix, M. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aPourbaix%2C+M+%22Atlas+of+electrochemical+equilibria+in+aqueous+solutions%2C+Ist+ed%22">Atlas of electrochemical equilibria in aqueous solutions, Ist ed</a>. , Pergamon Press. New York. 168-176 (1966).</li>
<li>Young, G. A., Scully, J. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((The+diffusion+and+trapping+of+hydrogen+in+high+purity+aluminum%5BTitle%5D)+AND+%22Acta+Materialia%22%5BJournal%5D)">The diffusion and trapping of hydrogen in high purity aluminum.</a> Acta Materialia. 46, 6337-6349 (1998).</li>
<li>Smith, S. W., Scully, J. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((The+identification+of+hydrogen+trapping+states+in+an+Al-Li-Cu-Zr+alloy+using+thermal+desorption+spectroscopy%5BTitle%5D)+AND+%22Metallurgical+and+Materials+Transactions+A%22%5BJournal%5D)">The identification of hydrogen trapping states in an Al-Li-Cu-Zr alloy using thermal desorption spectroscopy.</a> Metallurgical and Materials Transactions A. 31, 179-193 (2000).</li>
</ol>

The authors have nothing to disclose.

One important aspect of the FW procedure is the attachment of the two specimens to the magnetic stirrer. Because the center of the stirrer bar becomes the non-friction zone, it is best to avoid the attachment of the specimens at the center of the stirrer bar.
Control of the rotation speed of the stirrer bar is also important. When the speed is more than 240 rpm, it becomes difficult to maintain the reaction vessel on the stage of the magnetic stirrer. When the FW procedure is carried out at hi...

In general, aluminum base alloys have higher resistance to environmental hydrogen embrittlement than steel. The high resistance to hydrogen embrittlement of aluminum alloys is due to oxide films on the alloy surface blocking hydrogen entry. To evaluate and compare the high embrittlement sensitivity between aluminum alloys, hydrogen charging is usually performed prior to mechanical testing1,2,3,4,5,6,7,8,9,10,11,12,13,14,15,16,17. However, it is known that hydrogen charging aluminum is not easy, even when utilizing hydrogen charging methods such as cathodic charging15, slow strain rate deformation under humid air16, or hydrogen plasma gas charging17. The difficulty of hydrogen charging aluminum alloys is also due to the oxide films on the aluminum alloy surface. We postulated that higher amounts of hydrogen could be introduced into aluminum alloys if we could remove the oxide film continuously in water. Thermodynamically18, pure aluminum without oxide film reacts easily with water and generates hydrogen. Based on this, we have developed a new method of hydrogen charging of aluminum alloys based on the chemical reaction between water and non-oxide aluminum. This method is able to add high amounts of hydrogen into aluminum alloys in a simple way.

<table><tbody><tr><td>Air furnace</td><td>GC</td><td>QC-1</td><td></td></tr><tr><td>Aluminum alloy plates</td><td>Kobe Steel</td><td></td><td>Al/1.0 mass% Mg/0.8 mass% Si</td></tr><tr><td>Electric balance</td><td>A&amp;amp;D</td><td>HR-200</td><td></td></tr><tr><td>Glass container</td><td></td><td></td><td>Custom made</td></tr><tr><td>Magnetic stirrer</td><td>CORNING</td><td>PC-410D</td><td></td></tr><tr><td>Optical Comparator</td><td>NIKON</td><td>V-12B</td><td></td></tr><tr><td>pH meter</td><td>Sato Tech</td><td>PH-230SDJ</td><td></td></tr><tr><td>Quartz tube</td><td></td><td></td><td>Custom made</td></tr><tr><td>Rotary polishing machine</td><td>IMT</td><td>IM-P2</td><td></td></tr><tr><td>Secondary electrom microscope</td><td>JOEL</td><td>JSM-5310LV</td><td></td></tr><tr><td>Sensor gas chromatograph</td><td>FIS Inc.</td><td>SGHA</td><td></td></tr><tr><td>Silicon carbide emery paper</td><td>IMT</td><td>531SR</td><td></td></tr><tr><td>Tensile testing machine</td><td>Toshin Kogyo</td><td>SERT-5000-C</td><td></td></tr><tr><td>Tubular furnace</td><td>Honma Riken</td><td></td><td>Custom made</td></tr></tbody></table>

hydrogen charging of aluminum using friction in water

Hydrogen Charging of Aluminum using Friction in Water

A new method of hydrogen charging of aluminum was developed by means of a friction in water (FW) procedure. This procedure can easily introduce high amounts of hydrogen into aluminum based on the chemical reaction between water and non-oxide coated aluminum.

Hydrogen generation/absorption by the FW procedure 
Figure 2 shows the hydrogen generation behavior during the FW procedure of Al-Mg-Si alloys containing different amounts of iron from 0.1 mass % to 0.7 mass %. The specimen continuously emitted a high amount of hydrogen when the stirrer started to rotate. This suggests that hydrogen was generated by a chemical reaction caused by the friction between the alloy surface and water. In addition, the pH value of the water durin...

In order to introduce high amounts of hydrogen in aluminum and aluminum alloys, a new method of hydrogen charging was developed, called the friction in water procedure.

A new method of hydrogen charging of aluminum was developed by means of a friction in water (FW) procedure. This procedure can easily introduce high ...

hydrogen-charging-of-aluminum-using-friction-in-water

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Learn a novel friction-in-water method to charge aluminum alloys with hydrogen, overcoming surface oxide film challenges. This technique enables efficient hydrogen storage and embrittlement studies in materials science.

Hydrogen Charging of Aluminum using Friction in Water

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